CN104788116B - A kind of connector of zirconia-based ceramics and metal and attaching method thereof - Google Patents
A kind of connector of zirconia-based ceramics and metal and attaching method thereof Download PDFInfo
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- CN104788116B CN104788116B CN201410026240.9A CN201410026240A CN104788116B CN 104788116 B CN104788116 B CN 104788116B CN 201410026240 A CN201410026240 A CN 201410026240A CN 104788116 B CN104788116 B CN 104788116B
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Abstract
The invention provides connector of a kind of zirconia ceramics and metal and attaching method thereof, the connector includes the connector of ceramic member, metalwork, connection ceramic member and metalwork；The compound zirconia ceramic member that the ceramic member is the zirconia ceramics part that carburizing blacks or carburizing blacks；The fusing point of the metalwork is higher than 1000 DEG C；The connector is nickel-base alloy part.The zirconia ceramics of the present invention and the connector of metal meet the requirement of welding, but this programme has very big advantage in cost and convenience by the use of cheap nickel-base alloy as solder connection metal and ceramics.
Description
Technical field
The invention belongs to the connection area of metal and ceramics, more particularly to a kind of zirconia-based ceramics and the connector of technology
And attaching method thereof.
Background technology
In interconnection technique of the ceramics with metal, active metal welding is most widely used, and this kind of method must assure that
Activated solder has good wet performance and binding ability to the ceramics and metal that are connected.Be widely used at present have using Ti as
Active component, the Ag-Cu-Ti solders using Ag-Cu eutectics as matrix, carried out directly by metal with ceramics be bonded；Also one
Kind is then to be connected coated metal with soldered metal using solder first by ceramic surface metallization using Mo-Mn methods.
Contain more precious metal in Ag-Cu-Ti solders, therefore cost is higher, valuable product, it is applied
It is restricted to a certain extent；And Mo-Mn surface metalation methods are mainly used in aluminium oxide ceramics and combined oxidation aluminium base pottery
Porcelain, it is not used to zirconia ceramics surface.
The content of the invention
The present invention is noble metal used in existing metal and ceramic joining solder to solve, the high technical problem of cost,
Connector of a kind of cheap zirconia ceramics of solder and metal and attaching method thereof is provided.
The invention provides a kind of zirconia ceramics and the connector of metal, the connector include ceramic member, metalwork,
Connect the connector of ceramic member and metalwork；The zirconia ceramics part or carburizing that the ceramic member blacks for carburizing black compound
Zirconia ceramics part；The fusing point of the metalwork is higher than 1000 DEG C；The connector is nickel-base alloy part.
Present invention also offers the connection method of above-mentioned zirconia ceramics and metal, the connection method includes following step
Suddenly：
S1, by ceramics carry out blackening process, obtain carburizing nigrescence ceramic member；
S2, ceramic member that carburizing blacks, nickel-base alloy part, metalwork be put into connecting mold, the nickel-base alloy is shown in
One end contacted with ceramic member, the other end and metal pieces into contact；
S3, by connecting mold put in a vacuum furnace, carry out heating in vacuum weld to obtain the company of zirconia ceramics part and metal
Fitting.
The connector of zirconia ceramics and metal provided by the present invention, using cheap nickel-base alloy as solder connection
The combined oxidation zirconium base ceramics that zirconia ceramics and metal, the zirconia ceramics to black by nickel-base alloy to carburizing and carburizing black
There is good wetability, and to other ceramics（Such as aluminium oxide ceramics）There is no wetability, realize the direct welding of ceramics and metal.
Using cheap nickel-base alloy solder, cost substantially reduces；Realize zirconia ceramics and combined oxidation zirconium base ceramics and metal
Direct welding.Precious metal is not included in nickel-base alloy alloy.
Brief description of the drawings
Fig. 1 is the structural representation of the handset shell of embodiments of the invention 1.
Embodiment
In order that technical problem solved by the invention, technical scheme and beneficial effect are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only explaining
The present invention, it is not intended to limit the present invention.
The invention provides a kind of zirconia ceramics and the connector of metal, the connector include ceramic member, metalwork,
Connect the connector of ceramic member and metalwork；The zirconia ceramics part or carburizing that the ceramic member blacks for carburizing black compound
Zirconia ceramics part；The fusing point of the metalwork is higher than 1000 DEG C；The connector is nickel-base alloy part.
According to connector provided by the present invention, welding effect in order to better improve, it is preferable that the nickel-base alloy bag
The element and content contained be：
Nickel 77-90wt%,
Phosphorus 10-12wt%,
Other metals 0-13wt%.
According to connector provided by the present invention, the nickel-base alloy has no particular limits, and can be commonly used in the art
Various nickel-base alloys, such as one kind in nickel-phosphorus alloy, ambrose alloy phosphorus, nickel chromium triangle phosphorus.
According to connector provided by the present invention, it is preferable that on the basis of the gross weight of the ceramic member, the carbon contains
Measure as 2-4wt%.The compound zirconia ceramic member that the zirconia ceramics part or carburizing that carburizing blacks black, is that carbon vapor penetrates into
In the structure cell and cell gap of zirconia ceramics, a part exists with compound form, and a part exists in the form of carbon simple substance, by
Carbon content in the reason, the ceramic member will not be too many.
According to connector provided by the present invention, it is preferable that the compound zirconia ceramic member includes zirconium oxide and modification
Agent；Further, the modifying agent is at least one of yittrium oxide, magnesia and calcium oxide.
According to connector provided by the present invention, it is preferable that the volume hundred of zirconium oxide in the compound zirconia ceramic member
Fraction is 85-95%.The modifying agent main stabilization and toughening effect, modifying agent add it is too many if show be not oxidation
The performance of zircon ceramic, stablizes very little and the effect of toughness reinforcing is not strong.
According to connector provided by the present invention, the metalwork has no particular limits, as long as fusing point is more than 1000 DEG C
, such as at least one of copper piece, ironware and titanium part.
Present invention also offers the connection method of zirconia ceramics described above and metal, the connection method include with
Lower step：
S1, by ceramics carry out blackening process, obtain carburizing nigrescence ceramic member；
S2, ceramic member that carburizing blacks, nickel-base alloy part, metalwork be put into connecting mold, the nickel-base alloy is shown in
One end contacted with ceramic member, the other end and metal pieces into contact；
S3, by connecting mold put in a vacuum furnace, carry out heating in vacuum weld to obtain the company of zirconia ceramics part and metal
Fitting.
According to connection method provided by the present invention, it is preferable that the condition of heating in vacuum welding is：By the vacuum
When stove is warming up to 920-950 DEG C with 8-10 DEG C of programming rate per minute, 5-15 minutes are incubated.
According to connection method provided by the present invention, it is preferable that the vacuum of the vacuum drying oven is 10-2 -10-4Mpa。
According to connection method provided by the present invention, it is preferable that the method that the step S1 carries out ceramics blackening process
For：Ceramic powders are processed into workpiece base, workpiece base is placed in graphite powder, is then placed on and is heated in a vacuum furnace
1350-1550 DEG C, insulation 2-4 hours produce the ceramic member of carburizing nigrescence.
According to connection method provided by the present invention, it is preferable that also include cleaning step after the step S1；It is described
The method of cleaning is that the ceramic member that carburizing blacks is placed on into 10-20 minutes in ultrasonic environment.
The present invention is described in further detail below by specific embodiment.
Example below is to prepare metallic mobile phone shell：Because of technical requirements, the front and rear end of shell need to be insulated and disconnected.
The zirconia ceramics or combined oxidation zircon ceramic that the present embodiment blacks are used as connection transition zone as insulating barrier by the use of nickel-base alloy
To realize connection.As shown in figure 1,1- phone housings front end, 2- phone housings rear end, 3- ceramics, 4- nickel-base alloys.
Embodiment 1
Specifically preparation method is：
1. using synchronous sintering nigrescence method, zirconia ceramics powder is processed into workpiece base, by the white oxide zirconium of shaping
Workpiece base is placed in graphite powder, is then placed on and is heated to 1350 DEG C in a vacuum furnace, 2 hours of insulation obtain black oxygen
Change zircon ceramic.On the basis of the gross weight of the ceramic member, the content of the carbon is 2wt%；
2. the zirconia ceramics handled well is placed in the container of dress water, then it is placed in ultrasonic environment 20 minutes, removes
The dirt on black removal zirconia ceramics surface；
3. by zirconia ceramics workpiece, the nickel-base alloy of nigrescence after cleaning（Ni 90wt%, P 10wt%）, stainless steel bonnet
Front-end and back-end are put into a connecting mold, nickel-base alloy folded up between bonnet front end and nigrescence zirconia ceramics, blacked
Between zirconia ceramics and rear cover back-end, such as the position in Fig. 1；
4. the part to be welded put well is put in a vacuum furnace, it is 10 to be then evacuated to air pressure in stove-2During Mpa levels, it is entered
Row heating welding；
5. the temperature in vacuum furnace, which becomes, turns to 8 DEG C per minute, it is heated to being incubated 15 minutes at 920 DEG C；
6. weldment A1 is taken out after temperature is down to room temperature.
Embodiment 2
Specifically preparation method is：
1. using synchronous sintering nigrescence method, the yittrium oxide of 85vol% zirconia ceramics powder and 15vol% is processed into workpiece
Base, the white compound zirconia workpiece base of shaping is placed in graphite powder, is then placed on and is heated to 1550 in a vacuum furnace
DEG C, 2 hours of insulation obtain black combined oxidation zircon ceramic.On the basis of the gross weight of the ceramic member, the content of the carbon
For 2wt%；
2. the zirconia ceramics handled well is placed in the container of dress water, then it is placed in ultrasonic environment 10 minutes, removes
The dirt on black removal zirconia ceramics surface；
3. by zirconia ceramics workpiece, the nickel-base alloy of nigrescence after cleaning（Ni 88wt%, P 12wt%）, stainless steel bonnet
Front-end and back-end are put into a connecting mold, nickel-base alloy folded up between bonnet front end and nigrescence zirconia ceramics, blacked
Between zirconia ceramics and rear cover back-end；
4. the part to be welded put well is put in a vacuum furnace, it is 10 to be then evacuated to air pressure in stove-2During Mpa levels, it is entered
Row heating welding；
5. the temperature in vacuum furnace, which becomes, turns to 8 DEG C per minute, it is heated to being incubated 15 minutes at 920 DEG C；
6. weldment A2 is taken out after temperature is down to room temperature.
Embodiment 3
Specifically preparation method is：
1. using synchronous sintering nigrescence method, the magnesium oxide powder of 90vol% zirconia ceramics powder and 10vol% is processed into
Workpiece base, the white oxide zirconium workpiece base of shaping is placed in graphite powder, is then placed on and is heated to 1450 in a vacuum furnace
DEG C, 4 hours of insulation obtain black zirconia ceramics.On the basis of the gross weight of the ceramic member, the content of the carbon is
4wt%；
2. the zirconia ceramics handled well is placed in the container of dress water, then it is placed in ultrasonic environment 15 minutes, removes
The dirt on black removal zirconia ceramics surface；
3. by zirconia ceramics workpiece, the nickel-base alloy of nigrescence after cleaning（Ni 80wt%, P 10wt%, Cu10%）, after copper
Lid front-end and back-end are put into a connecting mold, nickel-base alloy is folded up between bonnet front end and nigrescence zirconia ceramics, hair
Between black zirconia ceramics and rear cover back-end；
4. the part to be welded put well is put in a vacuum furnace, it is 10 to be then evacuated to air pressure in stove-4During Mpa levels, it is entered
Row heating welding；
5. the temperature in vacuum furnace, which becomes, turns to 10 DEG C per minute, it is heated to being incubated 5 minutes at 950 DEG C；
6. weldment A3 is taken out after temperature is down to room temperature.
Embodiment 4
Specifically preparation method is：
1. using synchronous sintering nigrescence method, 95vol% zirconia ceramics powder and 5vol% calcium oxide are processed into workpiece base,
The white oxide zirconium workpiece base of shaping is placed in graphite powder, is then placed on and is heated to 1350 DEG C in a vacuum furnace, insulation
3 hours obtain black zirconia ceramics.On the basis of the gross weight of the ceramic member, the content of the carbon is 3wt%；
2. the zirconia ceramics handled well is placed in the container of dress water, then it is placed in ultrasonic environment 20 minutes, removes
The dirt on black removal zirconia ceramics surface；
3. by zirconia ceramics workpiece, the nickel-base alloy of nigrescence after cleaning（Ni 77wt%, P 10wt%, Cr 13wt%）, iron
Bonnet front-end and back-end are put into a connecting mold, nickel-base alloy is folded up between bonnet front end and nigrescence zirconia ceramics,
Between nigrescence zirconia ceramics and rear cover back-end；
4. the part to be welded put well is put in a vacuum furnace, it is 10 to be then evacuated to air pressure in stove-2During Mpa levels, it is entered
Row heating welding；
5. the temperature in vacuum furnace, which becomes, turns to 8 DEG C per minute, it is heated to being incubated 10 minutes at 920 DEG C；
6. weldment A4 is taken out after temperature is down to room temperature.
Embodiment 5
Specifically preparation method is：
1. using synchronous sintering nigrescence method, 92vol% zirconia ceramics powder, 5vol yittrium oxide and 3vol% magnesia are added
The white oxide zirconium workpiece base of shaping is placed in graphite powder into workpiece base, is then placed on and is heated in a vacuum furnace by work
1350 DEG C, 2 hours of insulation obtain black zirconia ceramics.On the basis of the gross weight of the ceramic member, the content of the carbon
For 2wt%；
2. the zirconia ceramics handled well is placed in the container of dress water, then it is placed in ultrasonic environment 20 minutes, removes
The dirt on black removal zirconia ceramics surface；
3. by zirconia ceramics workpiece, the nickel-base alloy of nigrescence after cleaning（Ni 90wt%, P 10wt%）, titanium bonnet front end
It is put into rear end in a connecting mold, nickel-base alloy is folded up between bonnet front end and nigrescence zirconia ceramics, black oxidation
Between zircon ceramic and rear cover back-end；
4. the part to be welded put well is put in a vacuum furnace, it is 10 to be then evacuated to air pressure in stove-3During Mpa levels, it is entered
Row heating welding；
5. the temperature in vacuum furnace, which becomes, turns to 8 DEG C per minute, it is heated to being incubated 15 minutes at 920 DEG C；
6. weldment A5 is taken out after temperature is down to room temperature.
Comparative example 1
The white oxide zircon ceramic without nigrescence is welded together with metal using Ag-Cu-Ti solders.Test workpiece
It is same as Example 1, the connection transition medium referred at 1 in 1 figure of experiment is changed to Ag-Cu-Ti solders, ceramics change into not
The white oxide zircon ceramic of nigrescence, other are identical.
Manufacture craft is：
1. the white oxide zircon ceramic workpiece sintered is placed in the container of dress water, ultrasonic environment is then placed on together
In 20 minutes, remove the dirt of ceramic surface；
2. one layer of Ag-Cu-Ti solder is applied in the outside of white oxide zircon ceramic workpiece two after cleaning, then by itself and metal
Bonnet front-end and back-end are put into a connecting mold；
3. the part to be welded put well is put in a vacuum furnace, when being then evacuated to that air pressure is 10-2 Mpa levels in stove, to it
Carry out heating welding；
4. the temperature in vacuum furnace, which becomes, turns to 8 DEG C per minute, it is heated to being incubated 10 minutes at 920 DEG C；
5. weldment CA1 is taken out after temperature is down to room temperature.
Performance test
Strength test
The handset shell A1-A5 that embodiment the obtains and handset shell CA 1 that comparative example 1 obtains is tested in electronic universal
Butt welding point carries out the test of tensile strength on machine, tension 19Mpa, the results are shown in Table 1.
Table 1
。
As can be seen from Table 1, the connector of zirconia ceramics of the invention and metal is used as by the use of cheap nickel-base alloy and welded
Material connection metal and ceramics, meet the requirement of welding, but this programme has very big advantage in cost and convenience.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (11)
1. the connector of a kind of zirconia ceramics and metal, it is characterised in that the connector includes ceramic member, metalwork, company
Connect the connector of ceramic member and metalwork；The composite oxygen that the ceramic member is the zirconia ceramics part that carburizing blacks or carburizing blacks
Change zircon ceramic part；The fusing point of the metalwork is higher than 1000 DEG C；The connector is nickel-base alloy part, and the nickel-base alloy includes
Element and content be：
Nickel 77-90wt%,
Phosphorus 10-12wt%,
Other metals 0-13wt%.
2. connector according to claim 1, it is characterised in that the nickel alloy is nickel-phosphorus alloy, ambrose alloy phosphorus, nickel chromium triangle phosphorus
In one kind.
3. connector according to claim 1, it is characterised in that on the basis of the gross weight of the ceramic member, the carbon
Content be 2-4wt%.
4. connector according to claim 1, it is characterised in that the compound zirconia ceramic member includes zirconium oxide and changed
Property agent；The modifying agent is at least one of yittrium oxide, magnesia and calcium oxide.
5. connector according to claim 4, it is characterised in that the volume of zirconium oxide in the compound zirconia ceramic member
Percentage is 85-95%.
6. connector according to claim 1, it is characterised in that the metalwork be copper piece, ironware and titanium part in extremely
Few one kind.
7. the preparation method of the connector of zirconia ceramics and metal described in claim 1-6 any one, it is characterised in that
The connection method comprises the following steps：
S1, by ceramics carry out blackening process, obtain carburizing nigrescence ceramic member；
S2, ceramic member that carburizing blacks, nickel-base alloy part, metalwork be put into connecting mold, the one of the nickel-base alloy part
End contacts with ceramic member, the other end and metal pieces into contact；
S3, by connecting mold put in a vacuum furnace, carry out heating in vacuum weld to obtain the connector of zirconia ceramics part and metal.
8. preparation method according to claim 7, it is characterised in that the condition of heating in vacuum welding is：By described in
When vacuum drying oven is warming up to 920-950 DEG C with 8-10 DEG C of programming rate per minute, 5-15 minutes are incubated.
9. preparation method according to claim 7, it is characterised in that the vacuum of the vacuum drying oven is 10-2 -10-4Mpa。
10. preparation method according to claim 7, it is characterised in that ceramics are carried out blackening process by the step S1
Method is：Ceramic powders are processed into workpiece base, workpiece base is placed in graphite powder, is then placed on and heats in a vacuum furnace
To 1350-1550 DEG C, insulation 2-4 hours produce the ceramic member of carburizing nigrescence.
11. preparation method according to claim 7, it is characterised in that also include cleaning step after the step S1；
The method of the cleaning is that the ceramic member that carburizing blacks is placed on into 10-20 minutes in ultrasonic environment.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410026240.9A CN104788116B (en) | 2014-01-21 | 2014-01-21 | A kind of connector of zirconia-based ceramics and metal and attaching method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410026240.9A CN104788116B (en) | 2014-01-21 | 2014-01-21 | A kind of connector of zirconia-based ceramics and metal and attaching method thereof |
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| CN105364284B (en) * | 2015-12-04 | 2017-08-08 | 西北工业大学 | A kind of zirconium oxide or the low temperature fast welding method for aoxidizing zirconium based composite material |
| CN110372410B (en) * | 2019-07-31 | 2021-08-24 | 成都工业学院 | Metal-ceramic composite material and preparation method thereof |
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2014
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Non-Patent Citations (2)
| Title |
|---|
| Zirconia to Ti-6Al-4V Braze Joint for Implantable Biomedical Device;Guangqiang Jiang et al.;《J Biomed Mater Res Part B: Appl Biomater》;20041020;第72B卷;摘要，图1，第317页右栏材料和方法部分第2段 * |
| 氧化锆陶瓷润湿及钎焊的研究进展;刘桂武 等;《稀有金属材料与工程》;20090430;第38卷;第406-410页 * |
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